반응 #74911

반응 방정식

Hydrogen chloride

5-chloro-1-indanone

chlorine

→

2,5-Dichloro-1-indanone

용매

acetic acid

반응 조건

후처리

1. 1
   기타to flow slowly into the solution at 10° C.
2. 2
   기타to come gradually to room temperature
3. 3
   workup.WAITAfter standing overnight
4. 4
   workup.ADDITIONthe solution is poured onto ice
5. 5
   추출the oil which separates out is extracted with acetic acid ethyl ester
6. 6
   workup.DISTILLATIONthe solvent is distilled off under reduced pressure
7. 7
   기타The oil which remains crystallizes on standing
8. 8
   기타The product can be recrystallized from petroleum ether

실험 절차

Hydrogen chloride gas is passed into a solution of 10.11 g (60 mmoles) of 5-chloro-1-indanone in 50 ml of glacial acetic acid at 10°-15° C. for 30 minutes. 4.25 g (60 mmoles) of condensed chlorine are then allowed to flow slowly into the solution at 10° C. and the mixture is allowed to come gradually to room temperature and is subsequently stirred for 3 hours. After standing overnight, the solution is poured onto ice, the oil which separates out is extracted with acetic acid ethyl ester and the solvent is distilled off under reduced pressure. The oil which remains crystallizes on standing. The product can be recrystallized from petroleum ether and then melts at 63°-66° C.

출처